CN115893892B - Two-dimensional high-alumina type micro-nano foil-shaped material for bauxite, and preparation process and application thereof - Google Patents
Two-dimensional high-alumina type micro-nano foil-shaped material for bauxite, and preparation process and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 86
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910001570 bauxite Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 44
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000011888 foil Substances 0.000 claims abstract description 13
- 239000011575 calcium Substances 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011593 sulfur Substances 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 10
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 7
- 239000004568 cement Substances 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 239000000725 suspension Substances 0.000 claims description 28
- 239000007790 solid phase Substances 0.000 claims description 25
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 22
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 18
- 239000000920 calcium hydroxide Substances 0.000 claims description 18
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 18
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000292 calcium oxide Substances 0.000 claims description 11
- 235000012255 calcium oxide Nutrition 0.000 claims description 11
- HSEYYGFJBLWFGD-UHFFFAOYSA-N 4-methylsulfanyl-2-[(2-methylsulfanylpyridine-3-carbonyl)amino]butanoic acid Chemical compound CSCCC(C(O)=O)NC(=O)C1=CC=CN=C1SC HSEYYGFJBLWFGD-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000004575 stone Substances 0.000 claims description 9
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 8
- RGKMZNDDOBAZGW-UHFFFAOYSA-N aluminum calcium Chemical compound [Al].[Ca] RGKMZNDDOBAZGW-UHFFFAOYSA-N 0.000 claims description 8
- 229910001424 calcium ion Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 229910052602 gypsum Inorganic materials 0.000 claims description 7
- 239000010440 gypsum Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- CWDGUDXMEXCVBN-UHFFFAOYSA-L aluminum;calcium;carbonate Chemical compound [Al+3].[Ca+2].[O-]C([O-])=O CWDGUDXMEXCVBN-UHFFFAOYSA-L 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims 1
- 229940009827 aluminum acetate Drugs 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 238000005054 agglomeration Methods 0.000 abstract description 13
- 230000002776 aggregation Effects 0.000 abstract description 13
- 239000006185 dispersion Substances 0.000 abstract description 8
- YMUYTQCKKRCJMP-UHFFFAOYSA-N aluminum;calcium;oxygen(2-) Chemical compound [O-2].[Al+3].[Ca+2] YMUYTQCKKRCJMP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000903 blocking effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 239000000654 additive Substances 0.000 description 9
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 230000000996 additive effect Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 229940037003 alum Drugs 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 229940103272 aluminum potassium sulfate Drugs 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000011398 Portland cement Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- YALHCTUQSQRCSX-UHFFFAOYSA-N sulfane sulfuric acid Chemical compound S.OS(O)(=O)=O YALHCTUQSQRCSX-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to the technical field of concrete admixture preparation, and particularly discloses a two-dimensional high-alumina type micro-nano foil material of a bauxite, and a preparation process and application thereof. The micro-nano foil-shaped material comprises the following raw materials in parts by weight: 35-40 parts of slow-release aluminum raw materials, 22-24 parts of slow-release sulfur raw materials, 15-18 parts of calcium raw materials, an alkaline pH regulator and water. Wherein: the slow-release aluminum raw material is a cross-linked body formed by an aluminum source and any one of polyacrylate, polyethylenimine, polyacrylamide and the like. The two-dimensional high-alumina type micro-nano aluminum-calcium oxide foil-shaped material prepared by the method has weak agglomeration, has good dispersion stability in water, and even if the agglomeration is carried out, the scale of the formed agglomeration is still in a micron level, so that the micro-nano foil-shaped material can fully realize blocking of capillary macropores in concrete after being doped into the concrete, the compactness of the concrete is increased, and the impermeability of the concrete is improved.
Description
Technical Field
The invention relates to the technical field of concrete admixture preparation, in particular to a two-dimensional high-alumina micro-nano foil-shaped material of a bauxite, and a preparation process and application thereof.
Background
The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art.
In large-scale underground construction projects such as underground bridges, subways, tunnels and the like, cast concrete is generally required to have high impermeability, so that the waterproof and moistureproof effects are achieved. The current common method for improving the impermeability of cement concrete in the market is to add air-entraining additives to make the concrete generate unconnected air bubbles, fine particles (such as superfine mineral powder) and lamellar materials such as metakaolin. However, when the air entraining admixture is excessively added (> 4%), a large amount of air bubbles are introduced, so that the strength of the cement concrete is obviously reduced, and the service life of the cement concrete is reduced. The mode of adding fine particles and lamellar materials has the particle rearrangement phenomenon, so that the fine particles and lamellar materials are difficult to ensure to be well dispersed in mixing water, and then enter into cement concrete to cut off communication holes and compact pores, which means that the mode of adding fine particles or lamellar materials to strengthen the impermeability of the cement concrete has lower efficiency and unsatisfactory effect.
Disclosure of Invention
In view of the above, the invention provides a two-dimensional high-alumina type micro-nano foil material of the bauxite and a preparation process thereof, which has good water dispersibility and can improve the impermeability of cement concrete after being doped into the concrete. In order to achieve the above object, specifically, the technical scheme of the present invention is as follows.
The invention discloses a two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material, which comprises the following raw materials in parts by weight: 35-40 parts of slow-release aluminum raw materials, 22-24 parts of slow-release sulfur raw materials, 15-18 parts of calcium raw materials, an alkaline pH regulator and 40-45 parts of water. Wherein: the slow-release aluminum raw material is a cross-linked body formed by an aluminum source and any one of polyvinyl alcohol, polyacrylate, polyethylenimine, polyacrylamide and the like.
Further, the proportion of the aluminum source to the polyvinyl alcohol, the polyacrylate, the polyethyleneimine or the polyacrylamide is 55 to 65 parts by weight: 35-45 parts by weight.
Further, the aluminum source comprises at least one of water-soluble aluminum salts such as aluminum sulfate, aluminum ammonium sulfate, alum and the like, and the crosslinking fusion of the aluminum source in the polyacrylate alcohol, the polyethyleneimine, the polyacrylamide and the like can effectively reduce the release rate of the Al 3+.
Further, the preparation process of the slow-release aluminum raw material comprises the following steps: and dissolving the aluminum source in water, adding any one of the polypropylene alcohol, the polyethylene imine, the polyacrylamide and the like, uniformly mixing to form a colloidal solution, and finally evaporating the water in the colloidal solution to obtain the granular slow-release aluminum raw material.
Further, the weight ratio of the aluminum source to the water is 0.25-0.6: 1. it should be understood that the aqueous solution of the aluminum source may also be used directly, thereby omitting the configuration process.
Further, the evaporating temperature is 90-125 ℃, and the evaporating time is constant weight.
Further, the slow-release type sulfur raw material comprises any one of phosphogypsum, fluorgypsum, desulfurized gypsum, gypsum pure reagent and the like, and can slowly release sulfate sulfur element to synthesize the two-dimensional high-aluminum type bauxite micro-nano foil-shaped material.
Further, the calcareous raw material includes any one of quicklime and slaked lime. In the invention, the characteristic that the quicklime reacts with water to form quicklime and the solubility of the quicklime in water is slightly soluble is utilized, so that the solution is always ensured to be in a saturated Ca 2+ state (namely Ca 2+ is always supplemented along with the progress of the reaction), thereby not only providing Ca 2+, but also carrying out chemical reaction with the slow-release aluminum raw material.
Further, the pH regulator comprises at least one of sodium carbonate, sodium bicarbonate, ammonia water and the like. Preferably, the pH regulator can regulate the pH value of a reaction system formed by the slow-release aluminum raw material, the slow-release sulfur raw material, the calcium raw material and water to 9.5-12.5. According to the invention, the two-dimensional high-alumina type micro-nano foil material of the bauxite is prepared in an alkaline reaction environment, so that the two-dimensional high-alumina type micro-nano foil material can be ensured to stably exist in the alkaline environment after entering cement concrete.
In a second aspect, the invention discloses a preparation process of the two-dimensional high-alumina type micro-nano foil-shaped material of the bauxite, which comprises the following steps:
(1) Mixing the calcareous raw material with water, and then adding the slow-release sulfur raw material to obtain a premix containing calcium ions and sulfate radicals for later use.
(2) Adding the slow-release aluminum raw material and an alkaline pH regulator into the premix, heating for reaction, separating out a solid phase product in a suspension obtained by the reaction after the reaction is completed, washing the solid phase product, and drying to obtain the two-dimensional high-aluminum type bauxite micro-nano foil-shaped material.
Further, in the step (2), the reaction temperature is 40-80 ℃ and the reaction time is 4-5 hours.
Further, in the step (2), the washing agent used in the washing may include any one of absolute methanol, absolute ethanol, and the like, to remove the reaction liquid remaining on the surface of the solid-phase product.
Alternatively, the method of separating out the solid-phase product in the suspension may include any one of suction filtration, centrifugation, and the like.
Further, in the step (2), the drying temperature is 50-70 ℃ and the drying time is constant weight.
Further, in the step (2), the length and the width of the micro-nano foil-shaped material are between 5 and 8 mu m, and the thickness is between 80 and 150 nm.
In a third aspect, the invention discloses application of the two-dimensional high-alumina type micro-nano foil-shaped material for the bauxite in cement or concrete. Preferably, the application mode is to blend the two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material into cement or concrete. Optionally, the mixing proportion of the two-dimensional high-alumina type bauxite micro-nano foil-shaped material in concrete is 6-8% of the mass of cement; or the mixing proportion of the two-dimensional high-alumina type bauxite micro-nano foil material in the cement is 2-4% of the mass of the cement.
Compared with the prior art, the technical scheme of the invention has at least the following beneficial effects:
in order to prepare the admixture capable of overcoming the defects of the methods of adding the air entraining admixture, adding the fine particles and adding the sheet material to improve the impermeability of the cement concrete, the method is mainly characterized in that firstly, the calcium material is provided to the reaction system in advance, but no target product is obtained, after analysis, side reactions are found to generate aluminum hydroxide precipitation and calcium sulfate precipitation (small amount of calcium hydroxide) or Ca (excessive amount of calcium hydroxide) under the conditions, and the materials cannot achieve the purposes after being added into the concrete, and the method is further explored, and the main reason is that the calcium material is firstly provided to the reaction system for providing sufficient Ca 2+, and then the slow-release aluminum material and the slow-release sulfur material are respectively released to the reaction system for low release of Al 3+ and sulfate, so that the side reactions are effectively avoided, and the two-dimensional high-aluminum-type micro-nano foil material is obtained.
The two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material prepared by the method has weak agglomeration, has good dispersion stability in water, and even if the agglomeration is carried out, the scale of the formed agglomeration is still in a micron level, so that the micro-nano foil-shaped material can fully block capillary macropores in concrete after being doped into the concrete, the compactness of the concrete is increased, and the impermeability is improved. Meanwhile, the cement concrete has the advantages that the cement concrete is free from harmful influence on the mechanical strength under the condition of large mixing amount, and the traditional superfine mineral powder or metakaolin and other fine particles and lamellar materials are easy to agglomerate after being mixed into the concrete, so that the cement concrete has small contribution to impermeability and can influence the mechanical strength of the cement concrete. This results in the admixture of ultrafine ore powder or metakaolin being kept at a low level, but the lower admixture gives less improvement in the performance of concrete, and the improvement in admixture is instead in contradiction of deteriorating the performance of concrete. The micro-nano foil-shaped material effectively overcomes the problems, and the reason is that: the micro-nano foil material is a soft agglomeration material, namely, agglomeration among materials is caused by hydrogen bonds formed by partial hydroxyl groups existing on the surface of the material, and the agglomeration can be rapidly dispersed by mechanical stirring and other modes after the micro-nano foil material is added into concrete due to weak binding force among the hydrogen bonds, so that the agglomeration state can not be continuously kept in the concrete.
In addition, the two-dimensional high-alumina type micro-nano aluminum calcium oxide foil material prepared by the method is used as a site for adhering C-S-H gel of a cement hydration product after being doped into cement concrete, so that the cement hydration is promoted, and the crack resistance of the cement concrete is improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
fig. 1 is a Scanning Electron Microscope (SEM) image of a two-dimensional high alumina type micro-nano foil-shaped material of a calix prepared in example 1 of the present invention.
Fig. 2 is a graph showing the agglomeration test effect of the two-dimensional high alumina type micro-nano foil material of the bauxite prepared in the embodiment 1 of the present invention.
Fig. 3 is a graph showing the Zeta potential test result of the two-dimensional high alumina type micro-nano foil-shaped material of the bauxite prepared in the example 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. The experimental procedures, which do not address the specific conditions in the examples below, are generally carried out under conventional conditions or under conditions recommended by the manufacturer.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The reagents or materials used in the present invention may be purchased in conventional manners, and unless otherwise indicated, they may be used in conventional manners in the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described herein are illustrative only.
Example 1
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) 60 parts by weight of aluminum sulfate was added to 100 parts by weight of water and stirred to sufficiently dissolve aluminum sulfate in water to form an aluminum sulfate solution. Then adding 38 parts by weight of polypropylene alcohol 2000 into the aluminum sulfate solution, stirring for 10min at a speed of 1000r/min by using a stirrer to form a colloidal solution, and then placing the colloidal solution into a high-temperature blast drying box at 100 ℃ for drying to constant weight, thus obtaining the slow-release aluminum raw material.
(2) Adding 16 parts by weight of quicklime into 42 parts by weight of water, and magnetically stirring for 30min to enable the quicklime to fully react with the water, so as to obtain a slaked lime suspension. Then adding 23.5 parts by weight of gypsum powder into the slaked lime suspension to obtain a premix containing calcium ions and sulfate radicals for later use.
(3) 37 Parts by weight of the slow-release aluminum raw material prepared in this example was added to the premix, and then sodium bicarbonate was added to adjust the pH of the reaction system to 11. Then heating the obtained alkaline reaction system in water bath, and reacting for 5 hours at 60 ℃ to obtain suspension.
(4) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly washing the solid phase product for 3 times by using absolute ethyl alcohol, and after the completion, placing the obtained solid phase product in a blast drying oven to be dried to constant weight at the temperature of 60 ℃ to obtain the two-dimensional high-alumina micro-nano foil-shaped additive material (refer to figure 1).
Example 2
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) 65 parts by weight of aluminum ammonium sulfate was added to 260 parts by weight of water and stirred to sufficiently dissolve aluminum ammonium sulfate in water to form an aluminum ammonium sulfate solution. Then adding 45 parts by weight of polyethyleneimine 9002-98-6 (with molecular weight of 3000) into the aluminum ammonium sulfate solution, stirring for 15min at a speed of 1000r/min by using a stirrer to form a colloidal solution, and then placing the colloidal solution into a high-temperature blast drying box at 90 ℃ to be dried to constant weight, thus obtaining the slow-release aluminum raw material.
(2) 15 Parts by weight of slaked lime is added into 40 parts by weight of water and magnetically stirred for 30 minutes to obtain slaked lime suspension. And then adding 22 parts by weight of desulfurized gypsum powder into the slaked lime suspension to obtain a premixed solution containing calcium ions and sulfate radicals for later use.
(3) 35 Parts by weight of the slow-release aluminum raw material prepared in this example was added to the premix, and then ammonia water was added to adjust the pH of the reaction system to 12.5. Then heating the obtained alkaline reaction system in water bath, and reacting for 4 hours at 80 ℃ to obtain suspension.
(4) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly cleaning the solid phase product for 5 times by using absolute ethyl alcohol, and after the completion, placing the obtained solid phase product in a blast drying oven to be dried to constant weight at the temperature of 70 ℃ to obtain the two-dimensional high-alumina micro-nano foil-shaped additive material of the bauxite.
Example 3
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) 55 parts by weight of alum was added to 140 parts by weight of water and stirred so that the alum was sufficiently dissolved in the water to form an aluminum potassium sulfate solution. Then adding 35 parts by weight of polyacrylamide (weight average molecular weight 1000 ten thousand) into the aluminum potassium sulfate solution, stirring for 15min at a speed of 1000r/min by using a stirrer to form a colloidal solution, and then placing the colloidal solution into a high-temperature blast drying oven at 125 ℃ for drying to constant weight, thus obtaining the slow-release aluminum raw material.
(2) Adding 18 parts by weight of quicklime into 45 parts by weight of water, and magnetically stirring for 30min to obtain a slaked lime suspension. And then adding 24 parts by weight of phosphogypsum powder into the slaked lime suspension to obtain a premix containing calcium ions and sulfate radicals for later use.
(3) 40 Parts by weight of the slow-release aluminum raw material prepared in this example was added to the premix, and then sodium carbonate was added to adjust the pH of the reaction system to 9.5. Then heating the obtained alkaline reaction system in water bath, and reacting for 5 hours at 40 ℃ to obtain suspension.
(4) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly cleaning the solid phase product for 3 times by using absolute ethyl alcohol, and after the completion, drying the obtained solid phase product in a blast drying oven at the temperature of 50 ℃ until the weight is constant, thus obtaining the two-dimensional high-alumina micro-nano aluminum-calcium carbonate foil-shaped additive material.
Example 4
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) Adding 16 parts by weight of quicklime into 42 parts by weight of water, and magnetically stirring for 30min to enable the quicklime to fully react with the water, so as to obtain a slaked lime suspension. Then adding 23.5 parts by weight of gypsum powder into the slaked lime suspension to obtain a premix containing calcium ions and sulfate radicals for later use.
(2) To the premix was added 37 parts by weight of aluminum sulfate, and then sodium bicarbonate was added to adjust the pH of the reaction system to 11. Then heating the obtained alkaline reaction system in water bath, and reacting for 5 hours at 60 ℃ to obtain suspension.
(3) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly cleaning the solid phase product for 3 times by using absolute ethyl alcohol, and drying the obtained solid phase product in a blast drying oven at the temperature of 60 ℃ until the weight is constant, thus obtaining the additive material.
Example 5
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) 65 parts by weight of aluminum ammonium sulfate was added to 26 parts by weight of water and stirred to sufficiently dissolve aluminum ammonium sulfate in water to form an aluminum ammonium sulfate solution. Then adding 45 parts by weight of polyethyleneimine 9002-98-6 (with molecular weight of 3000) into the aluminum ammonium sulfate solution, stirring for 15min at a speed of 1000r/min by using a stirrer to form a colloidal solution, and then placing the colloidal solution into a high-temperature blast drying box at 90 ℃ to be dried to constant weight, thus obtaining the slow-release aluminum raw material.
(2) 15 Parts by weight of slaked lime is added into 40 parts by weight of water and magnetically stirred for 30 minutes to obtain slaked lime suspension. And adding 22 parts by weight of sodium sulfate into the slaked lime suspension to obtain a premix containing calcium ions and sulfate radicals for later use.
(3) 35 Parts by weight of the slow-release aluminum raw material prepared in this example was added to the premix, and then ammonia water was added to adjust the pH of the reaction system to 12.5. Then heating the obtained alkaline reaction system in water bath, and reacting for 4 hours at 80 ℃ to obtain suspension.
(4) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly cleaning the solid phase product for 5 times by using absolute ethyl alcohol, and drying the obtained solid phase product in a blast drying oven at the temperature of 70 ℃ until the weight is constant, thus obtaining the additive material.
Example 6
A preparation process of a two-dimensional high-alumina type micro-nano foil-shaped material of a bauxite comprises the following steps:
(1) Adding 18 parts by weight of quicklime into 45 parts by weight of water, and magnetically stirring for 30min to obtain a slaked lime suspension. Then adding 24 parts by weight of sodium sulfate into the slaked lime suspension to obtain a premix containing calcium ions and sulfate radicals for later use.
(2) To the premix was added 40 parts by weight of alum, followed by addition of sodium carbonate to adjust the pH of the reaction system to 9.5. Then heating the obtained alkaline reaction system in water bath, and reacting for 5 hours at 40 ℃ to obtain suspension.
(3) And (3) carrying out suction filtration on the suspension to obtain a solid phase product, repeatedly cleaning the solid phase product for 3 times by using absolute ethyl alcohol, and drying the obtained solid phase product in a blast drying oven at the temperature of 50 ℃ until the weight is constant, thus obtaining the additive material.
Performance testing
1. Mixing six groups of C40 ordinary concrete, respectively doping the additive materials prepared in the above examples 1-6, wherein the doping amount is 7% of the mass of the cement, namely the mixing ratio of the examined C40 ordinary concrete is: 42.5 Portland cement: fly ash: sand: broken stone: water: water reducing agent: inventive material = 1:0.15:1.99:2.54:0.44:0.03:0.07. the test pieces corresponding to the above examples were tested for their properties such as 28d compressive strength, flexural strength, split tensile strength, shrinkage, and impermeability.
2. The three groups of C40 ordinary concrete are respectively doped with air entraining additives (comparative 1), the doping amount is 4% of the cement mass, the doping amount is 20% of the cement mass, the doping amount is metakaolin (comparative 3), and the doping amount is 7% of the cement mass. Test pieces were prepared by the same method as described above for performance test.
The results of the tests for each property are shown in the following table. The compression strength, the flexural strength, the splitting tensile strength and other mechanical properties are tested according to GB/T50081-2019 'test method Standard for physical mechanical Properties of concrete', and the shrinkage and the impermeability are tested according to GB/T50082-2009 'test method Standard for Long-term Properties and durability of common concrete'. From the test results in the following table, it can be seen that: compared with examples 4-6 and comparative examples 1-3, the two-dimensional high-alumina type bauxite micro-nano foil-shaped material prepared in examples 1-3 can be doped to better improve various properties of concrete.
3. Agglomeration test: the two-dimensional high alumina type micro-nano aluminum calcium carbonate foil-shaped material prepared in the embodiment 1 is dispersed in water in a test tube and uniformly stirred, and then a dispersion effect graph is acquired at three time points of standing for 24 hours, 72 hours and 168 hours, as shown in fig. 2. It can be seen that after long-time standing, the dispersion state of the two-dimensional high-alumina type micro-nano aluminum-calcium carbonate foil-shaped material in water is almost unchanged, and no obvious agglomeration sedimentation phenomenon occurs. This shows that the two-dimensional high-alumina type bauxite micro-nano foil-shaped material has good dispersion stability in water. The two-dimensional high-alumina type bauxite micro-nano foil material still has the dimension of micron order even though the two-dimensional high-alumina type bauxite micro-nano foil material is agglomerated, and can still keep good dispersibility.
The Zeta potential of the dispersion of the two-dimensional high alumina type micro-nano-calico foil-like material at rest for 168 hours in fig. 2 was also tested, and the result is shown in fig. 3. It can be seen that: the absolute value of Zeta potential is more than or equal to 40mV, which shows that the dispersion liquid has better stability, and further proves that the two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material has better dispersion stability in water.
The foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (16)
1. The two-dimensional high-alumina type micro-nano foil-shaped material for the bauxite is characterized by comprising the following raw materials in parts by weight: 35-40 parts of slow-release aluminum raw materials, 22-24 parts of slow-release sulfur raw materials, 15-18 parts of calcium raw materials, and 40-45 parts of alkaline pH regulator and water; wherein: the slow-release aluminum raw material is a cross-linked body formed by an aluminum source and any one of polyvinyl alcohol, polyacrylate alcohol, polyethylenimine and polyacrylamide; the aluminum source comprises at least one of aluminum sulfate, aluminum ammonium sulfate, aluminum nitrate and aluminum acetate;
the slow-release type sulfur raw material comprises any one of phosphogypsum, fluorgypsum, desulfurized gypsum and gypsum pure reagent;
The calcareous raw material comprises any one of quicklime and slaked lime.
2. The two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material according to claim 1, wherein the proportion of the aluminum source to polyvinyl alcohol, polyacrylate alcohol, polyethylenimine or polyacrylamide is 55-65 parts by weight: 35-45 parts by weight.
3. The two-dimensional high-alumina type micro-nano aluminum material according to claim 1, wherein the preparation process of the slow-release type aluminum raw material comprises the following steps:
Dissolving the aluminum source in water;
then adding any one of polyvinyl alcohol, polyacrylate, polyethyleneimine and polyacrylamide, and uniformly mixing to form a colloidal solution;
Finally evaporating the water in the colloidal solution to obtain the granular slow-release aluminum raw material.
4. The two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material according to claim 3, wherein the weight ratio of the aluminum source to the water is 0.25-0.6: 1.
5. The two-dimensional high-alumina type micro-nano aluminum-calcium carbonate foil-shaped material according to claim 3, wherein the evaporating temperature is 90-125 ℃ and the evaporating time is constant weight.
6. The two-dimensional high alumina type micro-nano foil-like material according to any one of claims 1 to 5, wherein the alkaline pH adjuster comprises at least one of sodium carbonate, sodium bicarbonate, and ammonia water.
7. The two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material according to claim 6, wherein the alkaline pH regulator regulates the pH value of a reaction system formed by the slow-release aluminum raw material, the slow-release sulfur raw material, the calcium raw material and water to 9.5-12.5.
8. The process for preparing the two-dimensional high-alumina type micro-nano foil-shaped material of the bauxite, as claimed in any one of claims 1 to 7, is characterized by comprising the following steps:
(1) Mixing the calcareous raw material with water, and then adding the slow-release sulfur raw material to obtain a premix containing calcium ions and sulfur elements for later use;
(2) Adding the slow-release aluminum raw material and an alkaline pH regulator into the premix, heating for reaction, separating out a solid phase product in a suspension obtained by the reaction after the reaction is completed, washing the solid phase product, and drying to obtain the two-dimensional high-aluminum type bauxite micro-nano foil-shaped material.
9. The process for preparing the two-dimensional high-alumina type micro-nano foil-shaped material of the bauxite, as claimed in claim 8, is characterized in that in the step (2), the reaction temperature is 40-80 ℃ and the reaction time is 4-5 hours.
10. The process for preparing a two-dimensional high-alumina type micro-nano foil material according to claim 8, wherein in the step (2), the washing agent used for washing comprises any one of absolute methanol and absolute ethanol.
11. The process for preparing the two-dimensional high-alumina type micro-nano foil-shaped material of the bauxite, which is characterized in that the method for separating the solid phase product from the suspension comprises any one of suction filtration and centrifugation.
12. The process for preparing the two-dimensional high-alumina type micro-nano foil-shaped material according to claim 8, wherein in the step (2), the drying temperature is 50-70 ℃ and the drying time is constant weight.
13. The process for preparing the two-dimensional high-alumina type micro-nano foil-shaped material of the invention as set forth in claim 8, wherein in the step (2), the length and the width of the micro-nano foil-shaped material are between 5 and 8 μm, and the thickness is between 80 and 150 nm.
14. The use of the two-dimensional high-alumina type micro-nano aluminum-calcium stone foil-shaped material obtained by the preparation process of any one of claims 8-13 in cement or concrete.
15. The use according to claim 14, wherein the two-dimensional high-alumina type micro-nano foil-shaped material is mixed in the concrete in a proportion of 6-8% of the mass of the cement.
16. The use according to claim 14, wherein the two-dimensional high alumina type micro-nano foil-like material is incorporated in the cement in a proportion of 2-4% of the mass of the cement.
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| DE19713229A1 (en) * | 1997-04-01 | 1998-10-08 | Merck Patent Gmbh | Bone cement paste containing antibiotics |
| CN103396027A (en) * | 2013-07-25 | 2013-11-20 | 北京市建筑工程研究院有限责任公司 | Preparation method of novel alkali-free liquid accelerator |
| CN105884240A (en) * | 2014-12-23 | 2016-08-24 | 上海绿源生态混凝土有限公司 | Additive special for green ecological concrete |
| CN111566071A (en) * | 2017-11-07 | 2020-08-21 | 霍夫曼绿色水泥技术有限公司 | Method for preparing ettringite binder for forming building materials |
| CN115215574A (en) * | 2022-07-11 | 2022-10-21 | 济南大学 | Aluminum-based concrete microcrack self-repairing material, composition, preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DE19713229A1 (en) * | 1997-04-01 | 1998-10-08 | Merck Patent Gmbh | Bone cement paste containing antibiotics |
| CN103396027A (en) * | 2013-07-25 | 2013-11-20 | 北京市建筑工程研究院有限责任公司 | Preparation method of novel alkali-free liquid accelerator |
| CN105884240A (en) * | 2014-12-23 | 2016-08-24 | 上海绿源生态混凝土有限公司 | Additive special for green ecological concrete |
| CN111566071A (en) * | 2017-11-07 | 2020-08-21 | 霍夫曼绿色水泥技术有限公司 | Method for preparing ettringite binder for forming building materials |
| CN115215574A (en) * | 2022-07-11 | 2022-10-21 | 济南大学 | Aluminum-based concrete microcrack self-repairing material, composition, preparation method and application thereof |
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